App.note_xrd-7.pdf

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B-XRD 1101

Temperature-controlled XRD measurement using MiniFlex with 2D detector and BTS 500 Introduction The MiniFlex benchtop X-ray diffractometer can be used with the HyPix-400 MF high-speed two-dimensional detector and the BTS 500 temperature-control attachment (manufactured by Anton Paar), which enables measurements from room temperature to 500°C. With this desktop system, you can observe a phase transition of a substance due to temperature change in real time.

Measurements and results The diffraction pattern of magnesium chloride hexahydrate (MgCl2・6H2O) was measured while increasing the temperature, using the MiniFlex benchtop X-ray diffractometer, a HyPix-400 MF two-dimensional detector and a BTS 500 temperature control attachment (Fig. 1). As the temperature rises, the specimen, which was a hexahydrate at room temperature, became a tetrahydrate at around 90°C, a dihydrate at around 140°C, a monohydrate at around 200°C, and magnesium chloride hydroxide (MgCl(OH)) at around 270°C. The phase transitions due to dehydration were observed (Fig. 2).

Mg Cl2 ( H2 O )6

10

20

2(°)

Mg Cl2 ・4 H2 O

30

10

20

2θ (deg)

RT

2(°)

30

Fig. 1: The BTS 500 and the HyPix-400 MF on the MiniFlex

0

Mg Cl2 ・2 H2 O

10

20

2θ (deg)

MgCl2・6H2O

91°C

MgCl2・4H2O

138°C

Mg Cl2 ・ H2 O

10

20

198°C

2(deg) (°) 2θ

30

MgCl2・H2O

2(°)

30

2θ (deg)

MgCl2・2H2O

Mg O H Cl

10

20

271°C

2(deg) (°) 2θ

30

MgCl(OH)

Fig. 2: Result of temperature-controlled XRD measurement of magnesium chloride hexahydrate

Recommended equipment ► Benchtop X-ray Diffractometer MiniFlex + 2D Detector HyPix-400 MF + Temperature Control Attachment BTS 500 (O1115en)

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